CN105040065A - Method for preparing neat porous anodic alumina film - Google Patents
Method for preparing neat porous anodic alumina film Download PDFInfo
- Publication number
- CN105040065A CN105040065A CN201510337096.5A CN201510337096A CN105040065A CN 105040065 A CN105040065 A CN 105040065A CN 201510337096 A CN201510337096 A CN 201510337096A CN 105040065 A CN105040065 A CN 105040065A
- Authority
- CN
- China
- Prior art keywords
- oxidation
- mixing solutions
- phosphoric acid
- aluminium flake
- alumina film
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Catalysts (AREA)
- ing And Chemical Polishing (AREA)
- Electrical Discharge Machining, Electrochemical Machining, And Combined Machining (AREA)
Abstract
The invention discloses a method for preparing a neat porous anodic alumina film. The method comprises the steps that firstly, a pretreated aluminum piece is placed in a mixed solution of phosphoric acid and oxalic acid, then first-time anodic oxidation is carried out to obtain an alumina film, and the alumina film is removed; second-time oxidation completely identical to the first-time oxidation in condition is carried out; the obtained alumina film is placed into a phosphoric acid solution, and pore-enlarging at different times is carried out; and through adjustment of oxidation voltage and pore-enlarging time, the highly-neat porous anodic alumina film with the pore pitch ranging from 348 nm to 500 nm and the pore diameter ranging from 72 nm to 400 nm is prepared. The oxalic acid content in the dilute phosphoric acid solution is adjusted, so that the anodic oxidation voltage value is improved, the regularity of alumina film pores is improved, and the range of the pore pitch is widened. The application of the alumina film to the field of preparation of neat micro-nano materials can be greatly expanded.
Description
Technical field
The invention belongs to technical field of electrochemistry, relate to a kind of preparation method of regular porous anodic alumina films, specifically about with the mixing solutions adding oxalic acid in dilute phosphoric acid for electrolytic solution, the method for the anodic alumina films of the adjustable on a large scale high-sequential of preparation pitch of holes and aperture.
Background technology
Porous anodic alumina films be a kind of cylindrical bore perpendicular to aluminium substrate and six side's continuous structures arranged in parallel each other, the advantages such as have large specific surface area, aperture is adjustable, and preparation technology is simple.In recent years, porous anodic alumina film receives increasing concern, has potential using value in a lot of field, as filtration, catalysis, sensing, bionical etc.Masuda and Satoh proposed the technology of secondary oxidation first in 1996, namely the pellumina that first time anodic oxidation obtains is removed, with orderly pit aluminium flake with the identical situation of first time oxidizing condition under carry out second time and be oxidized, suprabasil orderly pit when secondary oxidation to the effect being formed with guide of hole, therefore ordered structure (the MasudaH of anodised aluminium is obtained, SatohM.Jpn.J.Appl.Phys., 1996,35:L126-L129).
Under normal circumstances, anodizing of aluminium is many to be carried out in sulfuric acid, oxalic acid and phosphoric acid solution, because compare with other acid electrolyte, the pellumina order obtained in these three kinds of solution significantly improves.In the sulphuric acid soln of 0.3M, obtain the pellumina that pitch of holes is 63nm under 25V voltage conditions, in the oxalic acid solution of 0.3M, under 40V voltage conditions to pitch of holes be the pellumina of 100nm, in the phosphoric acid solution of 0.1M, under 195V voltage conditions, obtain the pellumina of 500nm.Weak point is the pitch of holes of alumina formwork is discontinuous, which greatly limits the range of application of pellumina.Patent CN101240440A discloses the technique that mixed acid anodic oxidation prepares the thick pellumina in high rigidity wide aperture, and the aperture of preparation is between 80-140nm, and the limited and order of the regulation range in aperture still has much room for improvement.Patent CN101603191A discloses a kind of method of adding acetic acid in phosphoric acid solution, makes the pellumina aperture of preparing between 200-300nm, but surface hole defect very irregularity, and pore size differs.Patent CN103147108A discloses a kind of pitch of holes of preparing in citric acid and oxalic acid solution at the adjustable multiaperture pellumina of 150-650nm, and the order that Problems existing remains hole is bad.So preparation pitch of holes and aperture comparatively large and can on a large scale in can the anodic oxidation aluminium formwork tool of continuously adjustable high-sequential be of great significance.
Summary of the invention
The object of the present invention is to provide and a kind ofly prepare pitch of holes and aperture continuously adjustabe and the technology of the porous anodic aluminium oxide of hole arrangement high-sequential on a large scale.The pitch of holes of obtained aluminum oxide film can within the scope of 348-500nm continuously adjustabe, aperture can within the scope of 72-400nm continuously adjustabe, hole arrangement high-sequential.
The gentle anonizing of employing of the present invention prepares the adjustable and method of the anodic alumina films of high-sequential in aperture, comprising:
(1) pre-treatment is carried out to rafifinal surface;
(2) aluminium flake obtained with step (1) is for anode, and titanium plate is negative electrode, carries out electrochemical etching, obtain the aluminium flake of surfacing in the mixing solutions of perchloric acid and dehydrated alcohol;
(3) aluminium flake obtained with step (2) is for anode, and titanium plate is negative electrode, in the mixing solutions of phosphoric acid and oxalic acid, carry out once oxidation;
(4) pellumina with aluminium substrate that step (3) obtains is placed on the aluminum oxide removing generation in the mixing solutions of chromium trioxide and phosphoric acid, obtains the aluminium flake of the regular pit of surface band;
(5) aluminium flake step (4) obtained, as anode, carries out secondary oxidation respectively when identical with once oxidation condition;
(6) after secondary oxidation, in the mixing solutions of hydrochloric acid and cupric chloride, remove aluminium substrate, can high-sequential be obtained and the continuously adjustable anodic alumina films of pitch of holes;
(7) pellumina that step (6) obtains is placed in phosphoric acid solution carries out expanding treatment, the continuously adjustable porous anodic aluminium oxide structure of bore dia can be obtained.
In described step (1), aluminium flake purity is 99.999%, and pre-treatment comprises the ultrasonic cleaning carrying out 5min in acetone, after cleaning-drying, be placed on 10min in the NaOH solution of 1mol/L, the natural oxidizing layer on removing surface, finally use washed with de-ionized water dry.
In described step (2), the volume ratio of perchloric acid and dehydrated alcohol is 1: 4, voltage 21V, and polishing time is 5min, and temperature is 0 ~ 5 DEG C.
In described step (3), once oxidation adds in the system that different content oxalic acid (0.03M-0.2M) is electrolytic solution in 1wt% phosphoric acid solution to carry out, each electrolyte system, optimum oxidation voltage (200V-150V) corresponding respective respectively, and the determination of optimal voltage is by improving constantly oxidation voltage to each given electrolytic solution until reaction occurs what punch-through was determined, optimum oxidation voltage is exactly the threshold value punctured, also be react the maximum voltage value that can normally carry out, temperature is 0 ~ 3 DEG C, and oxidization time is 1-4h.
In described step (4), the mixing solutions of chromium trioxide and phosphoric acid is configured by the mixing solutions of 18g/LCrO3 and 6wt%H3PO4 to form, and temperature is 60 DEG C.
In described step (6), the mixing solutions of hydrochloric acid and cupric chloride is by 10%HCl and 0.1mol/LCuCl
2mixing solutions configuration form, pitch of holes continuously adjustabe within the scope of 348-500nm of the porous anodic alumina template obtained, hole arrangement high-sequential.
In described step (7), the concentration of phosphoric acid is 5wt%, and reaming temperature is 30 DEG C, and the time is 0.5-3.5h, obtains bore dia continuously adjustable multiaperture pellumina within the scope of 72-400nm.
Beneficial effect of the present invention:
(1) the present invention adopts the mixing solutions adding oxalic acid in dilute phosphoric acid as electrolytic solution, and adding of oxalic acid makes temperature of reaction above zero carrying out, and has good stability;
(2) by the adjustment to mixing solutions mesoxalic acid content and corresponding optimum oxidation voltage, obtaining pitch of holes can the anodic alumina films of the high-sequential of adjustment continuously in 348-500nm;
(3) by carrying out expanding treatment in phosphoric acid solution, aperture continuously adjustable pellumina within the scope of 72-400nm can be obtained;
(4) the present invention is relative to preparing anodic alumina films merely in oxalic acid solution, improve the regulation range of pitch of holes, avoiding punch-through adjoint when simple phosphoric acid solution mesohigh is oxidized relative to preparing anodic aluminum oxide film to improve response voltage (reaching 200V) in simple phosphoric acid solution.
Accompanying drawing explanation
Fig. 1 is the sample F ESEM figure of embodiment 1, wherein Fig. 1 (a) is front FESEM figure (the pitch of holes 500nm of non-reaming, aperture is 130nm), Fig. 1 (b) schemes for back side FESEM, and the front FESEM that Fig. 1 (c) is reaming 3.5h schemes (aperture is 400nm);
Fig. 2 is the surperficial FESEM figure of sample (pitch of holes 470nm, aperture 108nm) the non-reaming of embodiment 2;
Fig. 3 is the surperficial FESEM figure of sample (pitch of holes 446nm, aperture 101nm) the non-reaming of embodiment 3;
Fig. 4 is the surperficial FESEM figure of sample (pitch of holes 393nm, aperture 96nm) the non-reaming of embodiment 4;
Fig. 5 is the surperficial FESEM figure of sample (pitch of holes 348nm, aperture 72nm) the non-reaming of embodiment 5;
Embodiment
Embodiment 1
Be 99.999% high-purity aluminium flake grease that ultrasonic cleaning 5min removing is surperficial in acetone by purity, use washed with de-ionized water subsequently, be then placed on 10Min in the NaOH solution of 1mol/L, the natural oxidizing layer on removing surface, finally use washed with de-ionized water dry; With pretreated aluminium flake for anode, titanium plate as negative electrode, liquor capacity ratio be 1: 4 perchloric acid and dehydrated alcohol in, voltage 21V, temperature 0 ~ 5 DEG C, carries out the electrochemical etching of 5min, obtains the aluminium flake of surfacing; The aluminium flake of polished finish is made anode, and titanium plate is as negative electrode, and with the 1wt% phosphoric acid solution adding 0.03M oxalic acid for electrolytic solution carries out once oxidation, oxidation voltage 200V, temperature is 0 ~ 3 DEG C, and oxidization time is 2h; The pellumina with aluminium substrate after once oxidation is placed on 18g/LCrO
3and 6wt%H
3pO
4mixing solutions in, remove the aluminum oxide of generation when 60 DEG C; The aluminium flake of the regular pit of surface band obtained is carried out secondary oxidation when identical with once oxidation condition; After secondary oxidation, at 10%HCl and 0.1mol/LCuCl
2mixing solutions in remove aluminium substrate, can obtain high-sequential pitch of holes is 500nm, and aperture is the anodic alumina films of 130nm, and its FESEM picture is shown in accompanying drawing 1 (a), (b); The pellumina obtained is placed on 5wt%H
3pO
4carry out expanding treatment 3.5h in solution, can obtain the porous anodic aluminium oxide structure that bore dia is 400nm, accompanying drawing 1 (c) is shown in by its FESEM picture.
Embodiment 2
Be 99.999% high-purity aluminium flake grease that ultrasonic cleaning 5min removing is surperficial in acetone by purity, use washed with de-ionized water subsequently, be then placed on 10Min in the NaOH solution of 1mol/L, the natural oxidizing layer on removing surface, finally use washed with de-ionized water dry; With pretreated aluminium flake for anode, titanium plate as negative electrode, liquor capacity ratio be 1: 4 perchloric acid and dehydrated alcohol in, voltage 21V, temperature 0 ~ 5 DEG C, carries out the electrochemical etching of 5min, obtains the aluminium flake of surfacing; The aluminium flake of polished finish is made anode, and titanium plate is as negative electrode, and with the 1wt% phosphoric acid solution adding 0.05M oxalic acid for electrolytic solution carries out once oxidation, oxidation voltage 190V, temperature is 0 ~ 3 DEG C, and oxidization time is 2h; The pellumina with aluminium substrate after once oxidation is placed on 18g/LCrO
3and 6wt%H
3pO
4mixing solutions in, remove the aluminum oxide of generation when 60 DEG C; The aluminium flake of the regular pit of surface band obtained is carried out secondary oxidation when identical with once oxidation condition; After secondary oxidation, at 10%HCl and 0.1mol/LCuCl
2mixing solutions in remove aluminium substrate, can obtain high-sequential pitch of holes is 470nm, and aperture is the anodic alumina films of 108nm, and accompanying drawing 2 is shown in by its FESEM picture.
Embodiment 3
Be 99.999% high-purity aluminium flake grease that ultrasonic cleaning 5min removing is surperficial in acetone by purity, use washed with de-ionized water subsequently, be then placed on 10Min in the NaOH solution of 1mol/L, the natural oxidizing layer on removing surface, finally use washed with de-ionized water dry; With pretreated aluminium flake for anode, titanium plate as negative electrode, liquor capacity ratio be 1: 4 perchloric acid and dehydrated alcohol in, voltage 21V, temperature 0 ~ 5 DEG C, carries out the electrochemical etching of 5min, obtains the aluminium flake of surfacing; The aluminium flake of polished finish is made anode, and titanium plate is as negative electrode, and with the 1wt% phosphoric acid solution adding 0.07M oxalic acid for electrolytic solution carries out once oxidation, oxidation voltage 180V, temperature is 0 ~ 3 DEG C, and oxidization time is 2h; The pellumina with aluminium substrate after once oxidation is placed on 18g/LCrO
3and 6wt%H
3pO
4mixing solutions in, remove the aluminum oxide of generation when 60 DEG C; The aluminium flake of the regular pit of surface band obtained is carried out secondary oxidation when identical with once oxidation condition; After secondary oxidation, at 10%HCl and 0.1mol/LCuCl
2mixing solutions in remove aluminium substrate, can obtain high-sequential pitch of holes is 446nm, and aperture is the anodic alumina films of 101nm, and accompanying drawing 3 is shown in by its FESEM picture.
Embodiment 4
Be 99.999% high-purity aluminium flake grease that ultrasonic cleaning 5min removing is surperficial in acetone by purity, use washed with de-ionized water subsequently, be then placed on 10Min in the NaOH solution of 1mol/L, the natural oxidizing layer on removing surface, finally use washed with de-ionized water dry; With pretreated aluminium flake for anode, titanium plate as negative electrode, liquor capacity ratio be 1: 4 perchloric acid and dehydrated alcohol in, voltage 21V, temperature 0 ~ 5 DEG C, carries out the electrochemical etching of 5min, obtains the aluminium flake of surfacing; The aluminium flake of polished finish is made anode, and titanium plate is as negative electrode, and with the 1wt% phosphoric acid solution adding 0.1M oxalic acid for electrolytic solution carries out once oxidation, oxidation voltage 170V, temperature is 0 ~ 3 DEG C, and oxidization time is 2h; The pellumina with aluminium substrate after once oxidation is placed on 18g/LCrO
3and 6wt%H
3pO
4mixing solutions in, remove the aluminum oxide of generation when 60 DEG C; The aluminium flake of the regular pit of surface band obtained is carried out secondary oxidation when identical with once oxidation condition; After secondary oxidation, at 10%HCl and 0.1mol/LCuCl
2mixing solutions in remove aluminium substrate, can obtain high-sequential pitch of holes is 393nm, and aperture is the anodic alumina films of 101nm, and accompanying drawing 4 is shown in by its FESEM picture.
Embodiment 5
Be 99.999% high-purity aluminium flake grease that ultrasonic cleaning 5min removing is surperficial in acetone by purity, use washed with de-ionized water subsequently, be then placed on 10Min in the NaOH solution of 1mol/L, the natural oxidizing layer on removing surface, finally use washed with de-ionized water dry; With pretreated aluminium flake for anode, titanium plate as negative electrode, liquor capacity ratio be 1: 4 perchloric acid and dehydrated alcohol in, voltage 21V, temperature 0 ~ 5 DEG C, carries out the electrochemical etching of 5min, obtains the aluminium flake of surfacing; The aluminium flake of polished finish is made anode, and titanium plate is as negative electrode, and with the 1wt% phosphoric acid solution adding 0.2M oxalic acid for electrolytic solution carries out once oxidation, oxidation voltage 150V, temperature is 0 ~ 3 DEG C, and oxidization time is 2h; The pellumina with aluminium substrate after once oxidation is placed on 18g/LCrO
3and 6wt%H
3pO
4mixing solutions in, remove the aluminum oxide of generation when 60 DEG C; The aluminium flake of the regular pit of surface band obtained is carried out secondary oxidation when identical with once oxidation condition; After secondary oxidation, at 10%HCl and 0.1mol/LCuCl
2mixing solutions in remove aluminium substrate, can obtain high-sequential pitch of holes is 348nm, and aperture is the anodic alumina films of 72nm, and accompanying drawing 5 is shown in by its FESEM picture.
Claims (7)
1. a preparation method for regular porous anodic alumina films, is characterized in that comprising the steps:
(1) pre-treatment is carried out to rafifinal surface;
(2) aluminium flake obtained with step (1) is for anode, and titanium plate is negative electrode, carries out electrochemical etching, obtain the aluminium flake of surfacing in the mixing solutions of perchloric acid and dehydrated alcohol;
(3) aluminium flake obtained with step (2) is for anode, and titanium plate is negative electrode, in the mixing solutions of phosphoric acid and oxalic acid, carry out once oxidation;
(4) pellumina with aluminium substrate that step (3) obtains is placed on the aluminum oxide removing generation in the mixing solutions of chromium trioxide and phosphoric acid, obtains the aluminium flake of the regular pit of surface band;
(5) aluminium flake step (4) obtained, as anode, carries out secondary oxidation respectively when identical with once oxidation condition.
(6) after secondary oxidation, in the mixing solutions of hydrochloric acid and cupric chloride, remove aluminium substrate, can high-sequential be obtained and the continuously adjustable anodic alumina films of pitch of holes;
(7) pellumina that step (6) obtains is placed in phosphoric acid solution carries out expanding treatment, the continuously adjustable porous anodic aluminium oxide structure of bore dia can be obtained.
2. preparation method according to claim 1, it is characterized in that, in described step (1), aluminium flake purity is 99.999%, pre-treatment comprises the ultrasonic cleaning carrying out 5min in acetone, after cleaning-drying, is placed on 10min in the NaOH solution of 1mol/L, natural oxidizing layer on removing surface, finally uses washed with de-ionized water dry.
3. preparation method according to claim 1, is characterized in that, in described step (2), the volume ratio of perchloric acid and dehydrated alcohol is 1: 4, voltage 21V, and polishing time is 5min, and temperature is 0 ~ 5 DEG C.
4. preparation method according to claim 1, it is characterized in that, in described step (3), once oxidation adds in the system that different content oxalic acid (0.03M-0.2M) is electrolytic solution in 1wt% phosphoric acid solution to carry out, each electrolyte system, optimum oxidation voltage (200V-130V) corresponding respective respectively, and the determination of optimal voltage is by improving constantly oxidation voltage to each given electrolytic solution until reaction occurs what punch-through was determined, optimum oxidation voltage is exactly the threshold value punctured, also be react the maximum voltage value that can normally carry out, temperature is 0 ~ 3 DEG C, oxidization time is 1-4h.
5. preparation method according to claim 1, is characterized in that, in described step (4), the mixing solutions of chromium trioxide and phosphoric acid is by 18g/LCrO
3and 6wt%H
3pO
4mixing solutions configuration form, temperature is 60 DEG C.
6. preparation method according to claim 1, is characterized in that, in described step (6), the mixing solutions of hydrochloric acid and cupric chloride is by 10%HCl and 0.1mol/LCuCl
2mixing solutions configuration form, pitch of holes continuously adjustabe within the scope of 348-500nm of the porous anodic alumina template obtained, hole arrangement high-sequential.
7. preparation method according to claim 1, is characterized in that, in described step (7), the concentration of phosphoric acid is 5wt%, reaming temperature is 30 DEG C, and the time is 0.5-3.5h, obtains bore dia continuously adjustable multiaperture pellumina within the scope of 72-400nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510337096.5A CN105040065B (en) | 2015-06-16 | 2015-06-16 | A kind of preparation method of regular porous anodic alumina films |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510337096.5A CN105040065B (en) | 2015-06-16 | 2015-06-16 | A kind of preparation method of regular porous anodic alumina films |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105040065A true CN105040065A (en) | 2015-11-11 |
| CN105040065B CN105040065B (en) | 2019-01-01 |
Family
ID=54447027
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510337096.5A Expired - Fee Related CN105040065B (en) | 2015-06-16 | 2015-06-16 | A kind of preparation method of regular porous anodic alumina films |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105040065B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109758789A (en) * | 2019-03-05 | 2019-05-17 | 大连理工大学 | A method of preparing super hydrophilic/underwater superoleophobic aluminium net |
| CN110241450A (en) * | 2019-07-19 | 2019-09-17 | 广东工业大学 | A kind of porous anodic alumina template and its preparation method and application |
| CN111051557A (en) * | 2017-08-29 | 2020-04-21 | 脸谱公司 | Aluminum alloy with visible grains and aluminum alloy colored by double anodization |
| CN113514106A (en) * | 2021-07-14 | 2021-10-19 | 天津工业大学 | Preparation method and application of multifunctional sensor for synchronously measuring temperature, pressure and humidity |
| CN113622011A (en) * | 2021-08-03 | 2021-11-09 | 天津科技大学 | Process method and device for preparing porous anodic aluminum oxide film |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1609283A (en) * | 2003-10-21 | 2005-04-27 | 东莞理工学院 | Process for producing ordered porous anodic alumina form |
| JP2008045170A (en) * | 2006-08-15 | 2008-02-28 | Kanagawa Acad Of Sci & Technol | Porous alumina having through-pore and production method therefor |
| CN101240440A (en) * | 2007-11-16 | 2008-08-13 | 苏州有色金属研究院有限公司 | Technique for preparing high-hardness large-aperture thick film by mixed acid anode oxidation |
| CN101603192A (en) * | 2009-07-14 | 2009-12-16 | 桂林理工大学 | A kind of method of utilizing commercial-purity aluminium to prepare porous anodic alumina films |
| CN102776542A (en) * | 2012-07-25 | 2012-11-14 | 华南理工大学 | Preparation method of anodized aluminum film of through hole |
| CN104213174A (en) * | 2014-07-24 | 2014-12-17 | 昆明理工大学 | Method for expanding size of nano hole of anodic aluminum oxide template |
-
2015
- 2015-06-16 CN CN201510337096.5A patent/CN105040065B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1609283A (en) * | 2003-10-21 | 2005-04-27 | 东莞理工学院 | Process for producing ordered porous anodic alumina form |
| JP2008045170A (en) * | 2006-08-15 | 2008-02-28 | Kanagawa Acad Of Sci & Technol | Porous alumina having through-pore and production method therefor |
| CN101240440A (en) * | 2007-11-16 | 2008-08-13 | 苏州有色金属研究院有限公司 | Technique for preparing high-hardness large-aperture thick film by mixed acid anode oxidation |
| CN101603192A (en) * | 2009-07-14 | 2009-12-16 | 桂林理工大学 | A kind of method of utilizing commercial-purity aluminium to prepare porous anodic alumina films |
| CN102776542A (en) * | 2012-07-25 | 2012-11-14 | 华南理工大学 | Preparation method of anodized aluminum film of through hole |
| CN104213174A (en) * | 2014-07-24 | 2014-12-17 | 昆明理工大学 | Method for expanding size of nano hole of anodic aluminum oxide template |
Non-Patent Citations (2)
| Title |
|---|
| 万国华: "孔间距大范围可调阳极氧化铝的制备", 《华南理工大学硕士学位论文》 * |
| 赵婷婷 等: "纳米多孔阳极氧化铝模板的制备方法及应用的研究进展", 《天津工业大学学报 》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111051557A (en) * | 2017-08-29 | 2020-04-21 | 脸谱公司 | Aluminum alloy with visible grains and aluminum alloy colored by double anodization |
| CN109758789A (en) * | 2019-03-05 | 2019-05-17 | 大连理工大学 | A method of preparing super hydrophilic/underwater superoleophobic aluminium net |
| CN109758789B (en) * | 2019-03-05 | 2021-12-03 | 大连理工大学 | Method for preparing super-hydrophilic/underwater super-oleophobic aluminum net |
| CN110241450A (en) * | 2019-07-19 | 2019-09-17 | 广东工业大学 | A kind of porous anodic alumina template and its preparation method and application |
| CN113514106A (en) * | 2021-07-14 | 2021-10-19 | 天津工业大学 | Preparation method and application of multifunctional sensor for synchronously measuring temperature, pressure and humidity |
| CN113622011A (en) * | 2021-08-03 | 2021-11-09 | 天津科技大学 | Process method and device for preparing porous anodic aluminum oxide film |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105040065B (en) | 2019-01-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105040065A (en) | Method for preparing neat porous anodic alumina film | |
| Zhang et al. | TiO2 nanotube arrays with a volume expansion factor greater than 2.0: Evidence against the field-assisted ejection theory | |
| Zhang et al. | Simulation of anodizing current-time curves and morphology evolution of TiO2 nanotubes anodized in electrolytes with different NH4F concentrations | |
| CN102220616B (en) | Method for preparing titanium dioxide nanotube array | |
| Zhang et al. | Bamboo shoot nanotubes with diameters increasing from top to bottom: Evidence against the field-assisted dissolution equilibrium theory | |
| CN103147108B (en) | A kind of anodic alumina films and preparation method thereof | |
| Zhang et al. | Rapid growth of TiO2 nanotubes under the compact oxide layer: Evidence against the digging manner of dissolution reaction | |
| CN103243370B (en) | A kind of two step anonizings prepare the method for ordered big hole anodic aluminum oxide film | |
| Zhang et al. | Growth of anodic TiO2 nanotubes in mixed electrolytes and novel method to extend nanotube diameter | |
| CN105088310A (en) | Preparation method of conical anodized aluminum oxide template | |
| CN101603192A (en) | A kind of method of utilizing commercial-purity aluminium to prepare porous anodic alumina films | |
| CN102041540A (en) | Anodic aluminum oxide template with three-dimensional gradual-changed hole array nanostructure and preparation method of anodic aluminum oxide template | |
| Li et al. | Comparative study on the anodizing process of Ti and Zr and oxide morphology | |
| CN104911668A (en) | Method for preparing nano taper-hole anodic aluminum oxide template | |
| CN104404566B (en) | A kind of to modify TiO 2nano-tube array is the ti-lead dioxide anode in middle layer and preparation method thereof and application | |
| Mendes et al. | Investigation of roughness and specular quality of commercial aluminum (6061 alloy) for fabrication of nanoporous anodic alumina films | |
| Yang et al. | Rapid growth of titanium oxide nanotubes under the critical breakdown voltage: Evidence against the dissolution reaction of fluoride ions | |
| CN104746129A (en) | Preparation method of immobilized single-crystal anatase TiO2 nanowire membrane layer | |
| CN102127788B (en) | Method for preparing overlarge crystal-cell porous pellumina | |
| Yu et al. | Morphology evolution of porous anodic alumina in mixed H3PO4/NH4F electrolytes | |
| Yan et al. | Essential distinction between one-step anodization and two-step anodization of Ti | |
| Ni et al. | Quantitative analysis of the volume expansion of nanotubes during constant voltage anodization | |
| Peng et al. | The relationship between the growth rate of anodic TiO2 nanotubes, the fluoride concentration and the electronic current | |
| CN102277607A (en) | Method for preparing through hole anode alumina film with controllable aperture and thickness | |
| CN104947167A (en) | Method for preparing porous anode aluminum oxide nanotemplate with two consistent faces |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20190101 Termination date: 20200616 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |